US2224352A - Method of processing wood for the rapid maturation of whisky and other alcoholic liquors and wines - Google Patents

Description

Patented Dec. 10, 1940' UNITED STATES PATENT OFFlCE' METHOD OF 05:22:12 WOOD FOR.

RAPID MATUBATION OF WHISKY OTHER. ALCOHOLIC LIQUORS AND Ernst "r. Krebs and Ernst 'r. Krebs, Jr.

, San Francisco, Calii.

No Drawing.

Serial No. 186.186

20 Claims.

I y This invention relates to a method of processing wood for the rapid maturation of whisky and other alcoholic liquors and wines.

It has been discovered that oak wood contains 5 cryptogamic spores which, when activated into profuse growth, have beneficial action on liquorsi is rich in tannase and it is rich in aminosuccinamides. The tannase hydrolizes the tannins in the oak wood, thereby forming principally gallic acid, and this isfinally oxidized into ellagic and other acids, which form their corresponding esters with the alcohols in the liquor or wines. Upon the addition of liquor or wine, the aminosuccinamide is dissolved and finally dissociated into succinic and succinamic acids and amino groups, and at the same time causes oxidation. The succinic and succinamic acids, as .well as the amino groups, form their corresponding esters.

While the cryp'togamic growth takes Place in the regular barrel-ageing process, it does so slowly, taking a period of years to mature the liquor or wine properly. By comminuting the wood to provide a large exposed surface area, and by activating the spores to rapid and abundant growth,- a large amOuntof tannase and aminosuccinamide is produced in a short period of time, and it is the abundant supply of these two constituents, and the ready access of the liquor to dissolve them, that brings about rapid maturation of the liquor or wine.

In our Patent No. 2,070,794, we depended upon the action of an emulsin complex to bring about rapid growth of the cryptogamic spores. We have now found that many vegetable hormones.

or chemicals having chemical properties similar to these hormones, may be used in great dilution with or without the use or an emulsin complex, to activate the cryptogamic spores into profuse and rapid growth. We have also discovered that if an emulsin complex and a hormone are used in conjunction, a very much greater dilution is possibleto bring about this profuse growth, and that if either the emulsin complex or a hormone is used alone, a stronger solution is required. The combination of the emulsin complex and the hormone is preferable as it is more economical ticularly indole compounds of these and other 5 acids and activated by dilute solutions of magnesium chloride, calciumchloride and/or alkaline iodides, and-to a lesser extent by other halides;

all for the one purpose of stimulating a cryptogamic growth from their spores in the oak wood 20 to furnish the two constituents which are essential in bringing about the so-called ageing changes in wines and liquors. These two constituents are the enzyme tannase secreted by the cryptogamic growth which hydrolyzes the tannins, and the aminosuccinamide constituent of the cryptogamic growth, which causes oxidation of the alcohols and furnishes the important amino, succinic and k succlnamic esters when it becomes dissociated in the alcoholic liquid. 80 The hormones or chemicals are used in very dilute solutions, with very dilute" solutions of an emulsin complex, or either can be used alone. For example, if the hormone used is an auxin or heteroauxin, one part will be dissolved in approximately 100,000 parts of magnesium chloride solution of the approximate strength of 1 part in 500 par-ts of water. The toasted comminuted wood is processed by adding a s'ufiicient amount of this solution to make the wood quite moist, 40 placing the same in a closed oak wood, glass, or other suitable container, in a moderately warm place, to remain from 2 to 4- weeks. The contents should fill only half or two-thirds of the container, sothat the comminuted wood'can be stirred every day or two by revolving the-container, thereby mixing the upper and less moistened wood with the more moist lower strata in the container. Every other day, beginning about the tenth day, a small sample of the processed Wood is macerated for 12 hours with about four or flve times its bulk volume of proof new whisky, and tested for complete tannin conversion and for acids. When three drops of a 1%. aqueous solution of" ferric chloride is added to 2 cc. of this extract, no blue color or precipitate should be produced, but a clear olive-green color should result, showing the extract is free of gallic acid. The extract should not contain less than 5 25 grams of acid to 100,000 cc. of the alcoholic extract, which acid is principally acetic acid. If the test proves the tannic and gallic acids of the wood have been fully converted, and the acid content of the new whisky macerated with the processed wood for 12 hours is up to at least the minimum standard, then it is ready for treatment of the new whisky. The processed comminuted wood is now placed in a closed vessel provided with a drain spout at the bottom, and about 15 three to six times (depending upon the wood) the bulk volume of new whisky is poured in and allowed to macerate for from 2 to 4 hours. It is then drained out, and immediately returned and allowed to macerate for from 10 to hours. These two macerations are done for the purpose of better extraction and mixing. The whisky is now drained and placed in an oak wood, glass or other suitable container and left to stand in a moderately warm place for to 90 days, when it will be ready to be bottled and sold as aged whisky.

In case the liquor is aged by this process in an oak' container, the container itself should be processed by spraying the solution of hormone'or chemical into the container under pressure, and maintaining the pressure for several days, to insure penetration of the solution into the wood. After the tightly closed oak wood container has set in a warm place for 30 to 90 days, the cryptogamic growth will be relatively profuse through a fair depth of the wood, and then the new whisky is to be placed in the processed oak wood container and allowed to remain in a warm place for 3 to 6 months. Containers of 10 to 20 gallon x 0 capacity have proven to be the best size, due to the relatively greater surface area exposed to the liquor than with large containers.

In case of new wine to be treated, this should have gone through the stages of alcoholic fermentation and have slightly entered the stage of acetic fermentation, to the point where it has a distinctly tart taste. For the treatment of wine, the processing of the oak wood container,.or the comminuted oak wood, is just the same as for to treating whisky, and the macerating process is just the same, but where the comminuted oak wood process is used, the proportion of new wine to the processed oak wood 'is much greater than in the case of whisky, and the wine should be filtered and bottled as soon as it is drained from the processed comminuted wood.

While in the example given a vegetable hormone has been described, it should be understood that an-emulsin complex and a hormone may be used 50 in conjunction, andthat a much greater dilution is then possible to bring about the same activation and profuse growth of the cryptogamic spores. On the other hand, a hormone alone or an emulsin complex alone may be used, but a stronger solution will be required. The combination of an emulsin complex and a hormone is preferable, as it is more economical and more efficacious. When an emulsin complex derived from the kernel of the fruit of Prunus armeniaca is used in combination with a hormone or with a chemical of the same or similar chemical groups as the hormone, the emulsin complex can be used in a solution of one part to 50,000 to 100,000 parts of magnesium chloride solution of a dilution of one part to 500 parts of water; andthe hormone, for

instance heteroauxin, can be used in a solution of one part to 1,000,000 parts or more of a solution of magnesium chloride of a solution of one part to 500 parts of water.

Magnesium chloride may be employed, and so may calcium chloride, and/or sodium iodide. Activation to a lesser degree is produced by other halides, as they function as activators or catalyzers for the emulsin complex and the hormones. The purpose of charring or toasting the oak, whether in comminuted form or not, is to dehydrate the tannins contained in the wood. When the wood is moistened with water during the first step of processing the wood, the tannins again become hydrated, which tannoid is apparently an intermediate tannoid body between gallic and ellagic acids, giving a blue reaction with ferric salts. When these are later acted upon by the enzyme complex rich in tannase, which is secreted by the cryptogamic growth, they are apparently oxidizedto ellagic acid, which again gives a green coloration with ferric salts.

When the new whisky or wine, containing ethyl and other alcohols, is added to the processed comminuted wood and allowedto macerate for several hours, all the changed products ofthe wood which aresoluble in hydro-alcoholic liquid, readily dissolve, leaving practically nothing behind but the cellulose of the wood. It is for this reason that only a few hours are required for the maceration of the hydro-alcoholic liquid in the processed comminuted wood. The whisky or wine may therefore be placed in any suitable container, such as charred oak barrels or containers made of glassware or the like, as it needs no further treatment with the oak wood.

The method produces the same biological (cryptogamic growth) and chemical phenomena which occur in the staves of the oak barrel containing whisky, wine or other alcoholic liquors,- in the regular barrel ageing process, with the advantages that this process gives a much more profuse cryptogamic growth, which is easily accessible to the hydroalcoholic solvent and which results in a greater production of aminosuccinamides, which in turn produces greater oxidation, aldehy'dation and esterification.

We have determined that many chemicals are able to produce a profuse cryptogamic growth, but the chemicals which particularly stimulate a profuse growth are many acids (particularly acetic,

butyli'c and propionic acids) combined with in-'- dole or other similar groups. We have also found that certain coal tar acids such as rmphthalene acids, and even furfural itself, will stimulate the cryptogamic growth. v v

The term "hormones as used in the claims is intended to cover any non-animal hormones, includirig those derived from roots, barks, woods,

herbsfileaves, seeds and plant products, or a syn thetic hormone or compound having spore acti vating. characteristics similar to the vegetable hormone.

Having thus described our invention, what we I claim and desire to secure by Letters Patent is:

1. In a method of processing oak wood to produce a prolific growth from its cryptogamic spores, the products of which growth promote oxidation, aldehydation and esterification during the ageing of spirituous liquors, those steps which consist in reducing the oak wood to a comminuted form and moistening the comminuted wood with a solution containing a growth-activating vegetable hormone.

2. In a method of processing oak wood to produce a prolific growth from its cryptogamic spores, the products of which growth promote oxidationbaldehydation and esterification during the ageing of spirituous liquors, those steps which consist in reducing the oak wood to a comminuted form and moistening the comminuted wood with a solution containing a growth-activating vegespores, the products of which growth promote oxidation, aldehydation and esterification during the ageing of spirituous liquors, those steps which consist in reducing the oak wood to a comminuted form and. moistening the comminuted wood with a solution containing a solution of a growthactivating vegetable hormone, an emulsin com,-

.plex and magnesium chloride.

5. In a method of processingoak 'wood to pro- .duce a prolific growth from its cryptogamic' spores, the products of which growth promote oxidation, aldehydation and esterification during the ageing of spirituous liquors, the step comprise ing treatingoak wood with a growth-activating vegetable hormone.

6. In a method of processing oak wood to produce a prolific growth from its cryptogamic spores, the products of which growth promote oxidation, aldehydation and esterification during the ageing of spirituous liquors, the step com-' prising treating oak wood with a growth-activating vegetable hormone and an emulsin complex.

7. In a method of processing oak wood to produce a prolific growth from its cryptogamic spores, the products of which growth promote oxidation, aldehydation and esterification during the ageing of spirituous liquors, the step which consists of impregnating the staves of an oak wood container with a solution containing a solution of a growth-activating vegetable hormone and magnesium chloride.

8. In a method of processing oak wood to produce a prolific growth from its cryptogamic spores, the products of which growth promote oxidation, aldehydation and esterification during the ageing of spirituous liquors, the step which consists of impregnating the staves of an oak wood container with a solution containing a solution of a growth-activating vegetable hormone, an emulsin complex and magnesium chloride.

9, In a method of processing oak wood to produce a prolific growth from its cryptogamic spores, the products of which growth promote I of processing oak wood to produce a prolific growth from its cryptogamic produce a prolific growth from its cryptog'amic spores, the products of which growth promote oxidation, aldehydation and esterificationv during the ageing of spirituous liquors and wines, the

steps which consist in reducing'the oak wood to a comminuted form, toasting the comminuted wood to dehydrate the tannins contained therein, and activating to prolific growth cryptogamic 'spores contained in the comminuted wood by moistening the wood with a-soiutiomcontaining a growth-activating vegetable hormone and an emulsin complex. I

11. ha method of processing oak wood to 1 produce a prolific growth from its cryptogamic spores, the products of which growthv promote oxidation, aldehydation and esterification during the ageing of "spirituous liquors and wines, the

steps which consist in reducing the oak wood to a comminuted form, toasting the comminuted wood to dehydratethe tannins contained therein,- and activating to prolific growth cryptogamia spores contained in the comminuted wood by moistening the wood with a solution containing a solution of a growth-activating vegetable hormone and magnesium chloride.

12. In a method of processing oak wood to produce a prolific growth from its cryptogamic spores, the products of which growth promote oxidation, aldehydation, and esterification during the ageing of spirituous liquors and wines, the steps which consist in reducing the oak wood toa comminuted form, toasting the comminuted wood to dehydrate the tannins contained therein,

of anindole compound of a lower fatty acid and derivatives thereof.

. 14."I'he method of ageing spirituous liquors I comprising treating the same with oak wood containing vegetable hormone activated spores.

15. The method of treating oak wood to producea prolific growth of its cryptogamic spores comprising treating the wood with a spore-activating hormone selected from the group consisting of a vegetable hormone and a synthetic hormone having spore activating characteristics similar to the vegetable hormone.

16. Oak wood containing cryptogamic spores activated into prolific growth, said growth being rich in aminosuccinarnides, said oak wood having its tannin compounds dissociated and being" adapted to produce in spirituous liquors, in a relatively short time, the same physical,-chemical, and biological phenomena as occur over a period of years when spirituous liquor is treated with normal unactivated oak wood.

17. Oak wood .containing cryptogamic spores activated into prolific growth, said growth being being rich in aminosuccinamides, said oak wood having its tannin compounds dissociated and being adapted to produce in spirituous liquors, in

ical, chemical, and biological phenomena as ocour over a period of years when spirituous liquor is treatedlwith normal unactivated oak wood.

20. Comminuted oak wood containing cryptogamic spores activated into prolific growth, said growth being rich in the enzyme tannase and in aminosuccinamides, said oak wood being adapted to produce in spirituous liquors, in a relatively short time, the same physical, chemical, and biological phenomena as occur over a period of years when spirituous liquor is treated with normal un- 10 activated oak wood. 4

ERNST T. KREIBS. ERNST T. KREBS, JR.